CN106975499B - 一种Ag@AgCl/rGO三明治纳米复合材料及其制备方法与应用 - Google Patents
一种Ag@AgCl/rGO三明治纳米复合材料及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种Ag@AgCl/rGO三明治纳米复合材料及其制备方法和作为等离子体增强型光催化剂的应用。本发明主要通过化学沉淀和光还原相结合的方法合成Ag@AgCl/rGO三明治纳米复合材料。本发明充分利用石墨烯的物理特性以及Ag@AgCl作为光催化剂的化学特殊属性，将两者的优良性能共同作用下，制备出具有阵列结构三维等离子体效应的Ag@AgCl/rGO三明治纳米复合材料，这种纳米复合材料有效地解决了石墨烯的聚集，提高了Ag@AgCl的耐久性，效率和活性。
Description
技术领域
本发明属于清洁可持续新型环境治理应用领域，特别涉及一种Ag@AgCl/rGO三明治纳米复合材料及其制备方法与其作为等离子体增强型光催化剂的应用。
背景技术
随着工业的发展，水污染极度严重，严重威胁了人类的健康。虽然现阶段处理废水的手段方法很多，比如：化学氧化法，生物方法等，虽然这些方法能够一定程度的处理污水，但是这些方法却有一定的缺陷。因此研制高效低廉的水处理技术迫在眉睫。光催化技术的一经发现就成为各领域的焦点，光催化是将光能转化为化学能的一种绿色化学反应。其中光催化剂有TiO2、ZnO等，这些光催化剂能够将大部分有机污染物转化为无害的CO2和水，然而也有一些缺陷以二氧化钛为例其只有在紫外光才能产生有效光响应，然而紫外光占太阳光的含量不足4％，因此开发新型的光催化材料具有重要的现实意义。
贵金属纳米颗粒由于其特殊的表面等离子体共振效应特殊性质。使其在光催化方面也得到了发展和应用特别是在Ag@AgCl核壳结构复合纳米颗粒中；作为新型光催化剂的Ag@AgCl光催化剂在可见光中表现出明显的等离子体共振效应从而显示有机污染物的可见光光催化降解的优异活性。同时石墨烯作为一种易合成的导电高分子材料，可以通过机械剥离法，化学气相沉淀法，氧化-还原法等制备。同时其拥有高比表面积，强机械以及导电性能在在太阳能电池，光催化，以及制氢储氢方面得到了广泛的应用，其中主要是从对环境的影响方面着手。
本发明的目的是针对现有技术的不足，提供一种Ag@AgCl/rGO三明治结构纳米复合材料及其光催化领域应用。这种纳米复合材料有效地解决了石墨烯的聚集，提高了Ag@AgCl的耐久性，效率和活性。
发明内容
本发明的目的在于针对现有技术的不足，提供一种Ag@AgCl/rGO三明治纳米复合材料及其化学催化应用。
本发明的目的是通过以下技术方案实现的：一种Ag@AgCl/rGO三明治纳米复合材料，包括石墨烯片层结构，所述石墨烯片之间通过摻杂在石墨烯片层之间的Ag@AgCl纳米颗粒进行粘结，Ag@AgCl纳米颗粒为核壳结构，石墨烯片与组成壳结构的Ag纳米颗粒之间通过Ag-C连接。
一种Ag@AgCl/rGO三明治纳米复合材料的制备方法，包括以下步骤：
(1)将氧化石墨烯醛基化，将醛基化后的氧化石墨烯分散到乙二醇中，获得浓度为1mg/ml的醛基化后的氧化石墨烯溶液。
(2)以乙二醇为溶剂，配制1*10-4mol/l的硝酸银溶液；
(3)将步骤1得到的氧化石墨烯溶液和步骤2得到的硝酸银溶液按照体积比3∶2混合，均匀搅拌并加入与Ag+等摩尔的NaCl溶液形成AgCl沉淀，得到AgCl/GO纳米复合材料溶液。
(4)将步骤3得到的溶液在500W紫外灯光照下进行还原10-30min，得到最终产物Ag@AgCl/rGO三明治结构纳米复合材料。
一种Ag@AgCl/rGO三明治纳米复合材料在光催化中的应用。
本发明的有益效果是：本发明Ag@AgCl/rGO三明治纳米复合材料由AgCl@rGO通过光还原和化学还原的相结合，其中紫外光的作用使AgCl部分还原成Ag颗粒，由于醛基的活性大，使Ag+首先与修饰醛基的氧化石墨烯上形成Ag晶种，乙二醇的加入使Ag晶种增大同时将氧化石墨烯还原为石墨烯，由于贵金属的其粘结性得到产物三明治Ag@rGO纳米复合结构。其中AgCl作为可以促进Ag颗粒的等离子体效应形成Ag@AgCl等离子体共振效应，银纳米颗粒作为一种粘结剂与石墨烯以Ag-C连接。Ag@AgCl特殊结构可以增强可见光等离子体共振性能，特别是AgCl包覆结构可以增强其等离子体共振性能。共振电子使得AgCl中的能级可以调控，增强光催化性能；三明治结构降低了Ag@AgCl与石墨烯的聚集，提高了催化材料的耐久性，效率和活性。同时还原氧化石墨烯作为良好的导体可以抑制电荷复合。作为非碳颗粒进入层中，石墨烯的层间距离将增加，导致层间范德华力减弱，导致层间范德华力减弱，从而降低团聚的可能性。同时，由于复合材料的三明治以及rGO高比面积大大提高对MO的还原活性。
附图说明
图1是实施例1制备的Ag@AgCl/rGO三明治纳米复合材料工艺示意图。
图2是实施例1制备Ag@AgCl/rGO三明治纳米复合材料的扫描电镜图SEM(a)和XRD图像(b)。
图3是实施例1制备Ag@AgCl/rGO纳米复合材料光催化降解亚甲基橙的光催化降解曲线(a)以及重复利用性能(b)；
图4为Ag@AgCl核壳结构形成示意图。
具体实施方式
下面结合实施例对本发明作进一步说明本发明的技术解决方案，这些实施例不能理解为是对技术解决方案的限制。
实施例1：
本实施例制备Ag@AgCl/rGO三明治纳米复合材料，具体包括以下步骤：
(1)将氧化石墨烯醛基化，将醛基化后的氧化石墨烯分散到乙二醇中，获得浓度为1mg/ml的醛基化后的氧化石墨烯溶液。
(2)以乙二醇为溶剂，配制1*10-4mol/l的硝酸银溶液；
(3)将步骤1得到的氧化石墨烯溶液和步骤2得到的硝酸银溶液按照体积比3∶2混合，均匀搅拌并加入与Ag+等摩尔的NaCl溶液形成AgCl沉淀，得到AgCl/GO纳米复合材料溶液。
(4)将步骤3得到的溶液在500W紫外灯光照下进行还原10-30min，得到最终产物Ag@AgCl/rGO三明治结构纳米复合材料。其中表层的AgCl通过光还原还原成银，构成Ag@AgCl核壳材料，如图4所示；GO通过乙二醇的还原性还原成为rGO；在还原过程中由于贵金属银的粘结性使Ag@AgCl与rGO以Ag-C键复合形成三明治结构。
图1为本发明制备的Ag@AgCl/rGO三明治结构纳米复合材料工艺示意图，从图1中可以很清晰的可以看出Ag@AgCl/rGO三明治结构的合成路线。图2为本发明制备的Ag@AgCl/rGO三明治结构纳米复合材料的扫描电镜图SEM(a)和XRD图像(b)，从图2a中可以看出，所述石墨烯片之间掺杂有纳米颗粒，结合2b和图4可知，该纳米颗粒为核壳结构的Ag@AgCl纳米颗粒；通过拉曼测试，图谱具有大量的1361cm-1的峰，表明材料中具有大量的Ag-C化学键，由此可以确定，石墨烯片与组成壳结构的Ag纳米颗粒之间通过Ag-C连接。
将上述制备的Ag@AgCl/rGO三明治结构纳米复合作为光催化剂进行光催化MO实验，具体为：量取50ml浓度20mg/L的甲基橙溶液，加入到150ml的玻璃反应器皿中，并均匀搅拌。称取30mg光催化剂加入到上述甲基橙溶液中，在黑暗下搅拌半个小时半个小时，目的是使光催化剂与染料分子达到吸附-解吸附平衡，同时验证其吸附能力大小。选取500w氙灯用于模拟紫外光可见光源，并放置在玻璃器皿的正上方10cm处，对混合溶液进行光照。记光照开始的时候t＝0，每隔一定时间取样4ml，离心取上层溶液有UV-vis测量最高峰吸光度分析光催化活性。
图3为本发明制备的在最佳条件下制备Ag@AgCl/rGO纳米复合材料光催化降解亚甲基橙的光催化降解曲线以及重复利用性能。光催化剂评价其好坏也可以从两个方面入手：(1)光催化速率的快慢：Ag@AgCl结构增强了可见光等离子体共振性能，由于AgCl包覆，使其共振性能增强；共振电子使得AgCl中的能级可以调控，增强光催化性能，阵列Ag@AgCl增加了协同强化性能；(2)光催化剂的稳定性。三明治结构降低了Ag@AgCl与石墨烯的聚集，提高了催化材料的耐久性，效率和活性。如图3a所示，在紫外光的照射下6分钟将MO降解完全，如图3b所示，经过10此循环利用后，Ag@AgCl/rGO纳米复合材料仍然保持95％以上的催化性能，这主要是由于Ag@AgCl核壳结构作为一个稳定的体系，同时更是受到rGO的保护。
本发明方法制备的Ag@AgCl/rGO三明治结构纳米复合材料制备方法简单，重复性高，可操作性强。这种纳米复合材料作为一种新型的光催化剂，表现出了较强光催化性能，以及光催化稳定性。
Claims (2)
1.一种Ag@AgCl/rGO三明治纳米复合材料的制备方法，所述Ag@AgCl/rGO三明治纳米复合材料包括石墨烯片层结构，石墨烯片之间通过掺杂在石墨烯片层之间的Ag@AgCl纳米颗粒进行粘结，Ag@AgCl纳米颗粒为核壳结构，石墨烯片与组成壳结构的Ag纳米颗粒之间通过Ag-C连接，其特征在于，包括以下步骤：
(1)将氧化石墨烯醛基化，将醛基化后的氧化石墨烯分散到乙二醇中，获得浓度为1mg/ml的醛基化后的氧化石墨烯溶液；
(2)以乙二醇为溶剂，配制1×10-4mol/l的硝酸银溶液；
(3)将步骤(1)得到的氧化石墨烯溶液和步骤(2)得到的硝酸银溶液按照体积比3∶2混合，均匀搅拌并加入与Ag+等摩尔的NaCl溶液形成AgCl沉淀，得到AgCl/GO纳米复合材料溶液；
(4)将步骤(3)得到的溶液在500W紫外灯光照下进行还原10-30min，得到最终产物Ag@AgCl/rGO三明治纳米复合材料。
2.一种权利要求1所述方法制备得到的Ag@AgCl/rGO三明治纳米复合材料在光催化中的应用。
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